CN111261737A - SnSe/Bi2Se3Nanosheet heterojunction and preparation method thereof - Google Patents
SnSe/Bi2Se3Nanosheet heterojunction and preparation method thereof Download PDFInfo
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Abstract
The invention discloses SnSe/Bi2Se3A nano-sheet heterojunction and a preparation method thereof, Bi2Se3Dispersing the nano-sheets on a substrate, opening an SnSe evaporation source, and performing vacuum evaporation to obtain SnSe/Bi2Se3A nanosheet heterojunction. SnSe/Bi prepared by the invention2Se3The thickness and the appearance of the heterojunction can be regulated and controlled according to the required characteristics, the substrate used in the experiment can also be selectively regulated and controlled, the preparation is independent of the type of the substrate, the experiment method is simple, the preparation can be carried out rapidly and massively, the environmental pollution is small, and the operation and the popularization are easy, so that the method has important research value and wide application prospect.
Description
Technical Field
The invention relates to the technical field of nano structures, in particular to SnSe/Bi2Se3Nanosheet heterojunction and method of making the same.
Background
Scientific research in recent years shows that the heterojunction can effectively separate photo-generated electron hole pairs and effectively regulate the transmission of electrons, and has important application value and application prospect in the technical field of photoelectrons.
Chinese patent CN109950138A discloses a nano-pillar array heterojunction and a preparation method thereof, firstly opening Bi2Te3Evaporation source for evaporating Bi on substrate2Te3Then turn off Bi2Te3Evaporating source, then mixing Sb2Te3The evaporation source is opened for vacuum evaporation and the product is collected on the substrate, thereby solving the technical defects that the prior art lacks a one-dimensional nano-pillar array heterojunction and utilizes the vacuum thermal evaporation technology to prepare the nano-pillar array heterojunction. However, the heterojunction preparation firstly needs vacuum thermal evaporation of a layer of thin film material, the growth of the heterojunction has certain dependence on the substrate, so that the application of the heterojunction is limited, and the experimental method is complicated.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defect and the defect that the preparation process of the existing heterojunction depends on the type of a substrate and provides SnSe/Bi2Se3The preparation method of the nano-sheet heterojunction comprises the steps of firstly preparing Bi2Se3The nano-sheets are dispersed on the substrate, and then evaporation is carried out by using SnSe as an evaporation source, so that the prepared nano-sheet heterojunction has no dependence on the substrate and the appearance and the thickness can be regulated and controlled.
Another object of the present invention is to provide a SnSe/Bi2Se3A nanosheet heterojunction.
The above purpose of the invention is realized by the following technical scheme:
SnSe/Bi2Se3The preparation method of the nanosheet heterojunction comprises the following steps:
s1, dissolving polyvinylpyrrolidone in a solvent, and adding Bi (NO)3)3、SeO2Mixing with oleic acid, performing hydrothermal reaction for 15h at 200 ℃, cooling to room temperature, washing and drying to obtain Bi2Se3Nanosheets; wherein the polyvinylpyrrolidone and Bi (NO)3)3、SeO2The mass ratio of (A) to (B) is 1-5: 0.3949: 0.1663, respectively;
s2, step S1Prepared Bi2Se3The nano-sheet is arranged on a substrate, and an SnSe evaporation source is opened for carrying out vacuum evaporation of SnSe to prepare SnSe/Bi2Se3A nanosheet heterojunction.
The invention adopts a hydrothermal method to prepare Bi firstly2Se3The nano-sheet is prepared into SnSe/Bi by adopting a multi-source high-vacuum thermal evaporation coating method2Se3Nanosheet heterojunction, heterojunction preparation is independent of substrate type, because heterojunction growth is in the existing Bi2Se3On the basis of the nano sheet, SnSe is evaporated and deposited on the nano sheet, and then a required nano sheet heterojunction is grown through deposition, so that the growth of the nano sheet heterojunction is irrelevant to the type of the substrate; in addition, the heterojunction prepared by the method does not need multiple complicated evaporation steps, the experimental method is simple, the heterojunction can be quickly prepared in large quantity, the environmental pollution is small, and the method is easy to operate and popularize, so that the method has important research value and wide application prospect.
Preferably, polyvinylpyrrolidone, Bi (NO) described in step S13)3、SeO2The mass ratio of (A) to (B) is 3: 0.3949: 0.1663.
polyvinylpyrrolidone (PVP) is used as a surfactant in the preparation process of the present invention.
Preferably, the solvent of step S1 is dimethylformamide.
Preferably, the substrate in step S2 is one of a silicon substrate, a semiconductor substrate, a dielectric substrate, or a metal substrate.
Preferably, the distance between the substrate and the evaporation source in the step S2 is 5-15 cm.
Preferably, the substrate temperature at the time of vacuum evaporation in step S2 is increased to 250 ℃.
Preferably, the evaporation source temperature in the vacuum evaporation in step S2 is increased to 350-450 ℃.
Preferably, the vacuum evaporation in step S2 is performed for 5-20 minutes.
Preferably, the temperature is reduced to 25-30 ℃ after the vacuum evaporation in the step S2 is finished.
Preferably, the pressure during vacuum evaporation is 5×10-5～7×10-5Pa。
Preferably, the specific operation method of step S2 is:
adding Bi2Se3Diluting the nanosheets, placing the diluted nanosheets on a substrate, placing SnSe in an evaporation source, adjusting the distance between the evaporation source and the substrate to be 5-15 cm, raising the temperature of the substrate to 250-300 ℃, raising the temperature of the SnSe evaporation source to 350-450 ℃, performing vacuum evaporation for 5-20 minutes, and cooling to 25-30 ℃ to obtain SnSe/Bi2Se3A nanosheet heterojunction.
The invention also protects the SnSe/Bi prepared by the preparation method2Se3A nanosheet heterojunction.
Compared with the prior art, the invention has the beneficial effects that:
the invention uses a certain amount of Bi synthesized in advance2Se3Diluting and dispersing the nanosheets on the substrate, weighing a certain amount of SnSe powder, placing the SnSe powder into an evaporation source, adjusting the distance between the evaporation source and the substrate to be 10cm, vacuumizing, raising the temperature of the substrate, raising the temperature of the SnSe evaporation source, evaporating after the experimental conditions are met, cooling and collecting a product; prepared SnSe/Bi2Se3The thickness and the morphology of the nano-sheet heterojunction can be regulated and controlled as required, the substrate used in the experiment can be regulated and controlled, the preparation is independent of the type of the substrate, the morphology and the thickness can be regulated and controlled according to the evaporation time and the temperature, the experiment method is simple, the preparation can be carried out rapidly and in large quantities, the pollution to the environment is small, and the operation and the popularization are easy, so that the method has important research value and wide application prospect.
Drawings
FIG. 1 shows SnSe/Bi obtained in example 12Se3X-ray diffraction pattern of nanosheet heterojunction, a1Is Bi2Diffraction peak of Se nanosheet, a2Is SnSe/Bi2Se3Diffraction peaks of the nanosheet heterojunction.
FIG. 2 shows Bi obtained in example 12Se3Scanning electron microscopy of the nanoplatelets, wherein (a) is at a magnification of 5k and (b) is at a magnification of 20 k.
FIG. 3 shows SnSe/Bi obtained in example 12Se3Scanning electron microscopy of a nanosheet heterojunction wherein (a) is at a magnification of 5k and (b) is at a magnification of 20 k.
FIG. 4(a) shows Bi2Se3The topography of the nano-sheet, (b) is a Se element distribution diagram, and (c) is a Bi element distribution diagram.
FIG. 5(a) shows SnSe/Bi of example 12Se3The topography of the nano-sheet heterojunction, (b) is a Se element distribution diagram, (c) is a Bi element distribution diagram, and (d) is a Sn element distribution diagram.
Detailed Description
The present invention will be further described with reference to specific embodiments, but the present invention is not limited to the examples in any way. The starting reagents employed in the examples of the present invention are, unless otherwise specified, those that are conventionally purchased.
Example 1
SnSe/Bi2Se3The preparation method of the nanosheet heterojunction comprises the following steps:
s1, adding PVP into 24mL of DMF, stirring uniformly, and then sequentially adding Bi (NO)3)3And SeO2In which PVP and Bi (NO)3)3、SeO2The mass ratio of (A) to (B) is 3: 0.3949: 0.1663, finally adding 12mLOA (oleic acid), stirring for 30 minutes, transferring into a reaction kettle, heating in an oven at 200 ℃ for 15 hours, naturally cooling to room temperature after reaction, washing the sample with alcohol and deionized water, drying the sample, and collecting to obtain Bi2Se3Nanosheets.
S2, adding Bi2Se3Diluting the nano-sheet with deionized water, dispersing on quartz substrate, placing SnSe powder in evaporation source, adjusting the distance between the evaporation source and the substrate to 10cm, and vacuumizing to 5 × 10-5Pa, raising the substrate temperature to 250 ℃, raising the SnSe evaporation source temperature to 450 ℃, and maintaining the air pressure at 5 x 10-5Pa, evaporating for 20 min; after the evaporation is finished, the temperature is reduced to 25 ℃ to collect SnSe/Bi on the substrate2Se3A nanosheet heterojunction.
Example 2
A kind ofSnSe/Bi2Se3The preparation method of the nanosheet heterojunction comprises the following steps:
S1.Bi2Se3the nanosheets were produced in the same manner as in example 1, except that polyvinylpyrrolidone and Bi (NO) were used in step S13)3、SeO2The mass ratio of (1): 0.3949: 0.1663.
s2, adding Bi2Se3Diluting and dispersing the nano-sheets on a silicon substrate, placing SnSe powder in an evaporation source, adjusting the distance between the evaporation source and the substrate to 10cm, and vacuumizing to 5 multiplied by 10-5Pa, raising the substrate temperature to 250 ℃, raising the SnSe evaporation source temperature to 450 ℃, and maintaining the air pressure at 5 x 10-5Pa, evaporating for 5 min; after the evaporation is finished, the temperature is reduced to 25 ℃ to collect SnSe/Bi on the substrate2Se3A nanosheet heterojunction.
Example 3
SnSe/Bi2Se3The preparation method of the nanosheet heterojunction comprises the following steps:
S1.Bi2Se3the nanosheets were produced in the same manner as in example 1, except that polyvinylpyrrolidone and Bi (NO) were used in step S13)3、SeO2The mass ratio of (A) to (B) is 2: 0.3949: 0.1663.
s2, adding Bi2Se3Diluting and dispersing the nano-sheets on a semiconductor substrate, placing SnSe powder in an evaporation source, adjusting the distance between the evaporation source and the substrate to 10cm, and vacuumizing to 5 multiplied by 10-5Pa, raising the substrate temperature to 250 ℃, raising the SnSe evaporation source temperature to 350 ℃, and maintaining the air pressure at 5 x 10-5Pa, evaporating for 20 min; after the evaporation is finished, the temperature is reduced to 25 ℃ to collect SnSe/Bi on the substrate2Se3A nanosheet heterojunction.
Example 4
SnSe/Bi2Se3The preparation method of the nanosheet heterojunction comprises the following steps:
S1.Bi2Se3the nanosheets were produced in the same manner as in example 1, except that polyvinylpyrrolidone and Bi (NO) were used in step S13)3、SeO2The mass ratio of (A) to (B) is 4: 0.3949: 0.1663.
s2, the preparation method of the step S2 is the same as that of the example 1.
Example 5
SnSe/Bi2Se3The preparation method of the nanosheet heterojunction comprises the following steps:
S1.Bi2Se3the nanosheets were produced in the same manner as in example 1, except that polyvinylpyrrolidone and Bi (NO) were used in step S13)3、SeO2The mass ratio of (A) to (B) is 5: 0.3949: 0.1663.
s2, the preparation method of the step S2 is the same as that of the example 1.
FIG. 1 shows SnSe/Bi obtained in example 12Se3An X-ray diffraction pattern of the nanosheet heterojunction. a is1Group data is Bi2Se3The diffraction spectrum of the nano-sheet is compared and analyzed with a standard card (PDF #33-0214), and the result shows that the obtained Bi is obtained2Se3The nano-sheet is a pure hexagonal crystal phase, the space group is R-3m, the peak shape of a diffraction spectrogram is relatively sharp, wherein the (015) diffraction peak position is strongest, which indicates that the prepared sample has relatively good crystallinity; a is2Group data are SnSe/Bi in example 12Se3Diffraction spectrum of nanosheet heterojunction, and1in contrast, a2Obvious SnSe diffraction peak (PDF #89-0232) appears, and the successful preparation of SnSe/Bi by the vacuum thermal evaporation technology is proved2Se3A nanosheet heterojunction.
FIG. 2 shows Bi obtained in example 12Se3Scanning electron microscopy images of the nanoplatelets at different magnifications. Bi is displayed according to the topography of a scanning electron microscope2Se3Is a large number of flaky morphology structures, Bi2Se3The dimension of the sheet reaches micron level, the thickness is below 100 nanometers, the surface is smooth, and the preparation of the one-dimensional Bi is proved2Se3Nanosheets.
FIG. 3 shows SnSe/Bi samples obtained in example 12Se3Scanning electron microscopy images of the nanosheet heterojunction at different magnifications. Shows in Bi according to the topography of a scanning electron microscope2Se3A layer of dense SnSe is uniformly deposited and grown on the nanosheets, and the surface roughness and the thickness of the nanosheets are increased, which indicates that the SnSe/Bi is successfully prepared2Se3A nanosheet heterojunction.
FIG. 4(a) shows Bi2Se3The topography of the nano-sheet, (b) is a Se element distribution diagram, and (c) is a Bi element distribution diagram. By the pair of Bi2Se3The nano-sheet is subjected to element distribution analysis, and the result shows that Bi is contained2Se3Se and Bi elements in the nanosheets are uniformly distributed.
FIG. 5(a) shows SnSe/Bi of example 12Se3The topography of the nano-sheet heterojunction, (b) is a Se element distribution diagram, (c) is a Bi element distribution diagram, and (d) is a Sn element distribution diagram. By pairing SnSe/Bi2Se3The element distribution analysis of the heterojunction is carried out, and the result shows that SnSe/Bi2Se3In the nano-sheet heterojunction, Se and Bi elements are uniformly distributed, and Sn element is in Bi2Se3The nano-sheets are also uniformly distributed on the positions, which proves that Bi is in2Se3A layer of SnSe is evenly deposited on the nano-chip, and finally SnSe/Bi is obtained2Se3A nanosheet heterojunction.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. SnSe/Bi2Se3The preparation method of the nanosheet heterojunction is characterized by comprising the following steps:
s1, dissolving polyvinylpyrrolidone in a solvent, and adding Bi (NO)3)3、SeO2Mixing with oleic acid, hydrothermal reacting at 200 deg.C for 15 hr, cooling to room temperatureThen washing and drying to obtain Bi2Se3Nanosheets; wherein the polyvinylpyrrolidone and Bi (NO)3)3、SeO2The mass ratio of (A) to (B) is 1-5: 0.3949: 0.1663, respectively;
s2, Bi prepared in the step S12Se3The nano-sheet is arranged on a substrate, and an SnSe evaporation source is opened for carrying out vacuum evaporation of SnSe to prepare SnSe/Bi2Se3A nanosheet heterojunction.
2. The method according to claim 1, wherein the polyvinylpyrrolidone of step S1, Bi (NO) are used3)3、SeO2The mass ratio of (A) to (B) is 3: 0.3949: 0.1663.
3. the method according to claim 1 or 2, wherein the solvent in step S1 is dimethylformamide.
4. The method according to claim 1, wherein the substrate in step S2 is one of a silicon substrate, a semiconductor substrate, a dielectric substrate, or a metal substrate.
5. The method according to any one of claims 1 to 4, wherein the distance between the substrate and the evaporation source in step S2 is 5 to 15 cm.
6. The method according to claim 5, wherein the substrate temperature at the time of vacuum evaporation in step S2 is increased to 250 ℃.
7. The method according to claim 5, wherein the evaporation source temperature in the step S2 of vacuum evaporation is increased to 350-450 ℃.
8. The method according to claim 5, wherein the step S2 is performed by vacuum evaporation for 5-20 minutes.
9. The method according to claim 5, wherein the vacuum evaporation pressure is 5 x 10-5～7×10-5Pa。
10. SnSe/Bi prepared by the preparation method of any one of claims 1 to 92Se3A nanosheet heterojunction.
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